US7507343B2 - Mixing and settling method and device in solvent extraction processes to recover high-purity products - Google Patents

Mixing and settling method and device in solvent extraction processes to recover high-purity products Download PDF

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US7507343B2
US7507343B2 US11/137,308 US13730805A US7507343B2 US 7507343 B2 US7507343 B2 US 7507343B2 US 13730805 A US13730805 A US 13730805A US 7507343 B2 US7507343 B2 US 7507343B2
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agitation
window
baffle
settler
turbines
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US20050218072A1 (en
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Daniel Martin San Lorenzo
Gustavo Diaz Nogueira
Maria Frades Tapia
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Tecnicas Reunidas SA
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Tecnicas Reunidas SA
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Assigned to TECNICAS REUNIDAS, S.A. reassignment TECNICAS REUNIDAS, S.A. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: NOGUEIRA, GUSTAVO DIAZ, SAN LORENZO, DANIEL MARTIN, TAPIA, MARIA FRADEX
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/04—Solvent extraction of solutions which are liquid
    • B01D11/0446—Juxtaposition of mixers-settlers
    • B01D11/0449—Juxtaposition of mixers-settlers with stationary contacting elements
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/04—Solvent extraction of solutions which are liquid
    • B01D11/0446—Juxtaposition of mixers-settlers
    • B01D11/0457—Juxtaposition of mixers-settlers comprising rotating mechanisms, e.g. mixers, mixing pumps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/04—Solvent extraction of solutions which are liquid
    • B01D11/0492—Applications, solvents used
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
    • B01D17/02—Separation of non-miscible liquids
    • B01D17/0208—Separation of non-miscible liquids by sedimentation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
    • B01D17/02—Separation of non-miscible liquids
    • B01D17/0208—Separation of non-miscible liquids by sedimentation
    • B01D17/0211—Separation of non-miscible liquids by sedimentation with baffles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
    • B01D17/02—Separation of non-miscible liquids
    • B01D17/0208—Separation of non-miscible liquids by sedimentation
    • B01D17/0214—Separation of non-miscible liquids by sedimentation with removal of one of the phases
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
    • B01D17/02—Separation of non-miscible liquids
    • B01D17/04—Breaking emulsions
    • B01D17/045—Breaking emulsions with coalescers

Definitions

  • This invention refers to a method and device perfecting the purification system used in extraction processes using organic solvents (hereinafter, SX) by means of mixers-settlers, as used for the recovery of metals and other products.
  • SX organic solvents
  • the invention includes new elements both with regards to equipment and operative methodology.
  • compartments any high-purity product, preferably metals and their salts, requiring SX technology with mixers-settlers, in which phases are mixed by stirring turbines and/or pumping in one or several mixing units, reactors or tandem compartments (hereinafter, compartments).
  • SX is a well-known separation technique, in which an impure aqueous solution containing the end product, ion or species (hereinafter, species) comes into contact with an organic solvent showing a special affinity with said species. After the complete mixing of the two phases, and once the matter has been transferred, it is separated for extraction of the end product.
  • the equipment typically used in this type of process consists of mixers and settlers. Each mixer-settler is called a “stage” in SX.
  • the mixer which may have several tandem compartments, has the function of dispersing the two phases to be mixed, to form an emulsion in order to favour transfer and obtain equilibrium.
  • the settler must be capable of re-separating the two components, organic phase and aqueous phase, forming the emulsion.
  • the most important parameters defining the operation are:
  • stirring intensity is largely determined by viscosity, surface tension and density differences between the phases. It is essential to identify the stirring intensity required, since too little leads to the formation of large droplets reducing the contact area and transfer, whereas too much causes the formation of stable emulsions and small droplets which are easily entrained by the other phase, with a negative impact on the purity of the end product obtained. Furthermore, is rotating stirring equipment is used, energy is concentrated on the borders, leading to a non-uniform droplet-size distribution.
  • the separation conditions depend both on the physical characteristics of the dispersed phases (differences of density, surface tension, viscosity, temperature, acidity, unitary speed) and on the intensity of the mix and the resulting droplet size.
  • the agitator in the first compartment of a stage mixer in an SX process normally has a two-fold function consisting of stirring and pumping the phases from the settlers in the adjacent stages, so its geometry is usually similar to that of a pump impeller.
  • the degree of agitation and pumping capacity largely depend on the size of the turbine, its stirring speed and its geometry. Normally, the organic and aqueous phases involved in the metal transfer reaction are easily and rapidly mixed with the thorough mixing of one phase with the other.
  • One type of radial agitation appropriate for both functions, gives the agitator a shear effect, especially on the borders of the turbine, and the greater the degree of this shear effect and agitation, the smaller are the droplets formed (and therefore the more difficult to decant).
  • the agitators in following mixer compartments have the function of maintaining the homogeneity, to provide time for the reaction according to the specific kinetics of each type of extraction and each phase involved. They can therefore be of the axial agitation (non-shear) type, with less agitation (size and/or speed).
  • the mix obtained in SX mixers is fed into settlers where the phases are separated by gravity, thanks to the different density of each phase.
  • This liquid-liquid separation is a dynamic process in which, since it is continuous, the speed and type of route of each phase affects the ease with which the resulting emulsion is broken, the surface area available and consequently the time of residence, temperature, acidity, etc.
  • the unitary speed of each phase may vary with the feed flow, including its possible recirculation and control of the position of the interface.
  • the ease with which the emulsion can be broken, for a given liquid temperature and characteristics, is not only affected by unitary speed but also be the type and degree of agitation obtained and the type of “internal elements”, which are especially designed barriers introduced in the flow to facilitate its distribution, homogenisation and lamination throughout the settler's geometry, or to facilitate an increase in the size of the droplets, therefore improving the decantation process.
  • stages Three stages are normally used in SX technology: extraction of the product or its species by an organic phase from an impure aqueous solution, washing to purify this organic phase and, finally, re-extraction of the purified species or product to a new aqueous phase.
  • stages there can be several mixers-settlers (stages) in serial formation, in which each phase (organic or aqueous) circulated against the current.
  • U.S. Pat. No. 4,925,441 contemplates a cascade of centrifuge contactors with intercommunications for phase mixing and separation, applicable to re-processing nuclear fuel.
  • U.S. Pat. No. 6,007,237 defends the action of a mix based on controlling agitation by the creation and propagation of vortex rings with a special agitator.
  • U.S. Pat. No. 4,551,314 (Amax, USA) covers a mixing system based on two tandem compartments, with different continuity conditions in the phase as an element favouring decantation.
  • U.S. Pat. No. 6,033,575 proposed a pre-separation of the dispersion in two independently decanted fractions.
  • This invention affects these last aspects: new designs, new internal elements and specific conditions.
  • the purpose of this invention is to obtain a drastic reduction in the entrainments of one phase in the other by reducing, depending on the phase, contamination of the organic phase with entrainments from the impure aqueous phase (aqueous entrainment in organic phase) or entrainments from the organic phase in the purified aqueous phase (organic entrainment in aqueous phase).
  • the proposed invention acts directly on one of the principal causes of impurity: entrainments from one phase in the other. This is reduced by acting both on the agitation system that provokes the emulsion created in the mixer and on the destruction of its consistency which persists along the dispersion band in the interface (settler).
  • a reduction in the quantity and consistency of the emulsion is obtained by jointly acting on the special design of the primary pump agitator (first compartment) and on its treatment due to the way of reducing this consistency throughout the rest of the compartments and, later, on the dispersion band in the settler with the introduction of systems and apparatus to reduce the quantity and persistence of the band.
  • the mix thus obtained overflows into the settler from the last compartment of the mixer through a communication channel.
  • the two phases are separated in the settler by means of a physical process in which the period of decantation until the emulsion becomes clear separated phases will depend, besides the specific operative conditions for each SX system selected (different density, temperature, type of mix, etc.), on the appropriate selection of unitary velocities for each phase and certain operative conditions which speed up the process. These conditions are not necessarily the same in all SX systems or in all settlers.
  • the emulsion is broken due to the collision and intersection of the disperse droplets, which break and grow in size when they move to rise or top, according to the relative density of each phase. More unitary velocity could cause more contacts, but not many because no turbulence is generated, whereas there would also be much less time for decantation, running the risk of overflow before this process is completed.
  • FIG. 1 shows a diagram of an SX installation which, in this case, shows eight stages or mixers-settlers, grouped into three typical stages of this type of installation: extraction, wash and re-extraction, with their interconnection and flows.
  • FIG. 2 shows a diagram of one of the mixers-settlers from FIG. 1 .
  • it is a mixer formed by four parallelopipedic tandem compartments, and a settler with details referring both to the position and shape of the traditional elements (distributor, flow buffers, recirculation system, and organic and aqueous phase overflows) and of new elements (baffle with and without window).
  • FIG. 3 shows a cross-section diagram of a primary agitator.
  • FIG. 4 shows a cross-section diagram of a secondary radial agitator.
  • FIG. 5 shows a cross-section diagram of a secondary axial agitator.
  • FIG. 6 shows a cross-section diagram of the mixer-settler from FIG. 2 , with details of the evolution of the emulsion in the mixer and how it is affected by the different internal elements in the settler.
  • FIG. 7 shows a front view of the baffles with windows.
  • FIG. 8 shows a front view of the baffles without windows.
  • Extraction stage 2 Wash stage 3 Re-extraction stage 4
  • Mixer consisting of a series of several compartments 5
  • Settler 6 Organic phase interconnection 7
  • Impure solution (fertile liquid) feed Residual (refined) impure solution 9
  • Aqueous phase feed to wash stage 10 Aqueous phase feed to re-extraction stage 11
  • Primary agitator 13 Secondary radial agitator 14
  • Secondary axial agitator 15 Communication channels between mixer compartments 15′ Communication channel upper overflow 15′′ Communication channel lower overflow 16
  • Turbine blades 17 Blunt edges on plates 18 Blunt edges on blades 19
  • Flow distributor 20 Flow buffer 21 Baffle with window 22 Window 23 Baffle without window 24
  • Emulsion 25 Upper overflow collection channel for the decanted organic phase 26
  • Lower overflow collection channel for the decanted aqueous phase 27 Final interface 28
  • Interface level control valve system 29 Recirculation system 30
  • Organic phase 31 Aqueous
  • FIG. 1 shows an installation to obtain a high-purity product by means of SX technology, consisting of three fundamental stages: extraction stage ( 1 ), wash stage ( 2 ) and re-extraction stage ( 3 ), each formed by a series of several mixers ( 4 )-settlers ( 5 ).
  • the series of mixers-settlers are connected by organic phase ( 3 ) interconnections ( 6 ) circulating and loading with the target product in the extraction stage ( 1 ), being washed in the wash stage ( 2 ) and unloading in the re-extraction stage ( 3 ).
  • the different aqueous phases fed to each stage flow in the opposite direction to the organic phase: an impure solution ( 7 ) (fertile liquid) containing the product of interest, which is extracted by the organic phase ( 30 ), leaving a residual impure solution ( 8 ) (refined); an aqueous phase to wash ( 10 ) which washes this loaded organic phase, and an aqueous phase to re-extraction ( 10 ), recovering the purified product from this organic phase ( 30 ) to obtain a purified aqueous solution ( 11 ) (aqueous extract).
  • FIG. 2 shows a diagram of this mixer ( 4 )-settler ( 5 ) in which, in this case, the mix of the organic phase ( 30 ) with the aqueous phases ( 31 ) and recirculation system ( 29 ) takes place in a mixer ( 4 ) consisting of a series of 4 compartments equipped with their respective primary agitators ( 12 ), secondary radial agitators ( 13 ) and secondary axial agitators ( 14 ), plus successive communication channels ( 15 ) consisting of successive mixer ( 4 ) compartments, with the fluid penetrating the communication channels ( 15 ) over an upper overflow ( 15 ′) located on the output side of the previous compartment, and beneath a lower overflow ( 15 ′′) located on the input side of the following compartment, which channels the mixture of the two phases from each compartment to the next independently.
  • a mixer 4 ) consisting of a series of 4 compartments equipped with their respective primary agitators ( 12 ), secondary radial agitators ( 13 ) and secondary axial agitators (
  • the secondary agitators ( 13 ) and ( 14 ) have turbines which keep the mixture agitated in the desired conditions for an appropriate material transfer and for the eventual separation process.
  • the primary agitator ( 12 ) turbine not only agitates, but also acts as a pump, aspiring each phase from the contiguous settlers and, if required, re-circulation from the settler itself.
  • the secondary agitator ( 13 ) and ( 14 ) turbines keep the phases mixed to complete this unit's function, with the possibility of varying mixing conditions for a better separation process.
  • the agitation conditions have to progressively decrease in the series of compartments with a view to, keeping the two phases agitated, reduce its intensity and aggressiveness, thus preparing the emulsion to facilitate settling and the grouping together of the smaller droplets.
  • these compartments can be intercommunicated with wide overflows ( 15 ) to facilitate the gradual reduction of the degree of agitation.
  • the settler ( 5 ) has both conventional flow distributor ( 19 ) systems, flow buffers ( 20 ), upper overflow collection channel for the decanted organic phase ( 25 ), lower overflow collection channel for the decanted aqueous phase ( 26 ), re-circulation system ( 29 ), interface level control valve system ( 28 ) and new elements consisting of a baffle with ( 21 ) and without a window ( 23 ).
  • both the primary agitator ( 12 ) and the secondary agitators ( 13 ) and ( 14 ) are equipped with blunt edges on the blades ( 18 ) and blunt edges on the plates ( 17 ), and this is irrespective of the number and arrangement of the blades ( 16 ).
  • These turbines avoid an excessive shear rate during agitation, inhibiting the secondary dispersion responsible for the formation of small droplets created from the large droplets originally produced during primary dispersion.
  • FIG. 6 shows how the emulsion ( 24 ) of the two phases flows from the last mixer ( 4 ) compartment and is finally fed into the settler ( 5 ).
  • This emulsion ( 24 ), a mixture of the organic phase ( 30 ) and the aqueous phase ( 31 ), is subject to a conventional flow distributor ( 19 ) system and another with the same purpose, homogeneously distributed over the surface of the settler, and one or two flow buffers ( 20 ) which buffer the flow.
  • the emulsion ( 24 ) behaves like a third phase with disappears over time inside the settler ( 5 ).
  • baffle with a window ( 21 ) and, further downstream, the baffle without a window ( 23 ), both around 500 mm high are installed cross-wise to the flow along the width of the settler, in the interface area and, as indicated by the evolution of the emulsion ( 24 ) in the interface, this improves phase separation and reduces entrainment.
  • These new units consist of independent elements aligned or installed on posts or columns anchored in the settler in order to favour their installation and maintenance in large settlers. Several of these units can even be installed in parallel if required by the specific conditions of the installation. Their relative position can also vary according to the stage (mixer-settler) considered, to obtain maximum efficacy.
  • baffles ( 21 ) and ( 23 ) made up of a series of modular units as shown in FIGS. 7 and 8 , and supported from beneath, are positioned cross-wise to the flow, covering the entire width of the settler ( 5 ).
  • the agitator turbines have a diameter of between 0.2 and 0.7 of the circular diameter equivalent to the cross section (of the circle of the same cross section) of the mixer compartment, with the degree of agitation decreasing from 50 rps 3 /sq.ft. to 0.5 rps 3 /sq.ft.
  • the height of the baffles is between 10% and 90% of the total height of the phases, and the opening of the baffles with windows is between 10% and 90% of their total surface area.
  • each stage of the same process extraction ( 1 ), wash ( 2 ) or re-extraction ( 3 )
  • Each SX process, and each stage in particular, requires optimisation for its specific objectives.
  • This improvement is general for each and every one of the typical stages of a solvent extraction process and, in relative terms with regards to its absence, more effective the more difficult is the natural decantation of the system on which it is applied.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Extraction Or Liquid Replacement (AREA)
  • Mixers Of The Rotary Stirring Type (AREA)
US11/137,308 2002-11-28 2005-05-25 Mixing and settling method and device in solvent extraction processes to recover high-purity products Active 2027-03-16 US7507343B2 (en)

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WOPCT/ES02/00565 2002-11-28
PCT/ES2002/000565 WO2004047946A1 (es) 2002-11-28 2002-11-28 Método y dispositivo de mezcla y sedimentacíon en procesos de extracción con disolventes para la recuperación de productos de gran pureza

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EP (1) EP1566208B1 (de)
CN (1) CN100354020C (de)
AU (1) AU2002358814A1 (de)
BR (1) BR0215956B1 (de)
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US20120018376A1 (en) * 2009-03-27 2012-01-26 Outotec Oyj Apparatus and method for removing impurities in connection with liquid-liquid extraction of copper
WO2012142648A1 (en) * 2011-04-20 2012-10-26 Hatch Associates Pty Ltd Distribution array for use in a settler area of a mixer-settler
US20130292341A1 (en) * 2012-05-07 2013-11-07 Freeport-Mcmoran Corporation System and method for separating liquid mixtures
US20150151218A1 (en) * 2012-06-26 2015-06-04 Outotec (Finland) Oy Method of manufacturing a solvent extraction settler and solvent extraction settler
US20150151460A1 (en) * 2012-06-26 2015-06-04 Outotec (Finland) Oy Method of manufacturing a separation fence and separation fence
US20150190734A1 (en) * 2012-06-26 2015-07-09 Outotec (Finland) Oy Solvent extraction settler arrangement
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US9631254B2 (en) 2012-06-26 2017-04-25 Outotec (Finland) Oy Solvent extraction method and solvent extraction settler
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US10190188B2 (en) 2012-11-25 2019-01-29 Turbulent Technologies Ltd. Mixing method and device for solvent extraction, especially in hydrometallurgical processes
WO2014094793A1 (en) * 2012-12-19 2014-06-26 Flsmidth A/S Apparatus and method for solvent extraction processing
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JP7430377B2 (ja) * 2019-06-19 2024-02-13 国立研究開発法人日本原子力研究開発機構 液液系での抽出分離による特定物質の製造装置

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CN100354020C (zh) 2007-12-12
MXPA05005650A (es) 2005-07-26
WO2004047946A1 (es) 2004-06-10
BR0215956A (pt) 2005-09-13
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AU2002358814A1 (en) 2004-06-18
EP1566208A1 (de) 2005-08-24

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